Blue sulfur dye and process of making same.



UNITED STATES Patented June 21 1904.

PATENT OFFICE.

ERNST MATHE, OF HOOHST-ON-THE-MAIN, GERMANY, ASSIGNOR TO FARBWVERKE, VORM. MEISTER, LUCIUS & BRIINING, OF HOGHST- ON-THE-MAIN, GERMANY, A CORPORATION OF GERMANY.

BLUE SULFUR DYE AND PROCESS OF MAKING SAME.

SPECIFICATION forming part of Letters Patent No. 763,193, dated June 21, 1904. Application filed March 30, 1904. Serial No. 200,794. (No specimens.)

To all whom it may concern:

Be it known that I, ERNST MATHE, Ph. D., chemist, a citizen of the Empire of Germany, residing at HOchst-on-the-Main, Germany, have invented certain new and useful Improvements in the Manufacture of a Blue Sulfurized Dyestuff, of which the following is a specification.

Diparaoxyphenyl para paral diamidodiphenylamin crystallizes when pure in the form of colorless leaflets, which melt at about 208 centigrade. This substance may be obtained by simultaneously oxidizing parapara1 diamidodiphenylamin and phenol or diphenylamin and para-amidophenol, both in molecular proportions of one to two, or by the action of quinonechlorimid on diphenylamin in molecular proportions of two to one. In any of these cases indophenol is obtained, which on being reduced yields dipara-oxy phenyl-para-parmdiamidodiphenylamin.

Example: Three hundred parts of the base of dipara-oxyphenyl para paral diamiclodiphenylamin are boiled for six hours in a reflux apparatus with eight hundred parts of crystallized sodium sulfid and three hundred and forty parts of sulfur and four hundred parts of glycerin, the temperature then being 100 to 110 centigrade. The evolution of hydrogen sulfid occurs already at 80 centigrade, and the base dissolves gradually. The

mass is then diluted with water, reboiled, and filtered. Air is introduced into the green filtrate, whereupon thedyestufl is precipitated. It is then filtered and dried.

Having now described my invention, what I claim is 1. The manufacture of a blue dyestuff from dipara-oxyphenyl para-para1 diamidodiphenylamin, which consists in heating this substance with sodium sulfid and sulfur for some time to 100 to 120 centigrade and in precipitating the dyestuff thus obtained from the mass diluted with Water, substantially as set forth.

2. As new product, a blue dyestuif from dipara-oXyphenyl-parapara1-diamidodiphenylamin as herein described, being when dry a dark-blue powder of metallic luster, insoluble in water, alcohol, ether, benzene, glacial acetic acid and dilute acids, soluble in dilute alkali lye with a blue, in concentrated sulfuric acid with a green color; the green solution of the dyestuff in sodium-sulfid solution dyeing cotton fast indigo-blue shades.

In testimony that I claim the foregoing as my invention I have signed my name in presence of two subscribing witnesses.

ERNST MATHE.

Witnesses:

ALFRED BRISBOIS, JOSEPH FLAcH. 

